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Method for detecting rhodium in water phase of olefin hydroformylation reaction system catalyzed by water-soluble rhodium-phosphine complex

A detection method and reaction system technology, applied in color/spectral property measurement, measurement devices, instruments, etc., can solve the problems of high cost, expensive instruments, difficult industrial production analysis and detection, etc., achieve high accuracy, reduce instrument costs, The effect of shortening the digestion time

Pending Publication Date: 2021-07-16
成都欣华源科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In CN105572104A, the inductively coupled plasma method was used to measure the rhodium content in the rhodium-containing organic solution, and in CN104634773A, the inductively coupled plasma emission spectrometry was used to measure the rhodium content in the triphenylphosphine-rhodium complex, but the instrument was expensive and cost High, difficult to apply to analysis and detection in industrial production
[0010] It can be seen that there is no relevant report about the assay method of the aqueous phase rhodium content in the water-soluble rhodium-phosphine complex catalyzed olefin hydroformylation reaction process, and it remains to be further developed.

Method used

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  • Method for detecting rhodium in water phase of olefin hydroformylation reaction system catalyzed by water-soluble rhodium-phosphine complex
  • Method for detecting rhodium in water phase of olefin hydroformylation reaction system catalyzed by water-soluble rhodium-phosphine complex
  • Method for detecting rhodium in water phase of olefin hydroformylation reaction system catalyzed by water-soluble rhodium-phosphine complex

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] (1) Digestion of samples: Use a pipette to accurately pipette 1mL of rhodium-containing aqueous phase catalyst solution, place it in a 250mL beaker, evaporate it on a heating plate at about 80°C until there is no obvious steam, add 10mL of concentrated sulfuric acid, and raise Digestion was carried out at heated temperature for 120 minutes. After the digestion is completed, continue to heat, evaporate the sulfuric acid to a nearly dry state, add 3mL of concentrated nitric acid after cooling, continue to heat until the solution becomes colorless and transparent, and cool down.

[0080] (2) Test sample preparation: transfer the sample into a 100mL volumetric flask, and dilute to volume with 1% nitric acid solution. Use a pipette to accurately pipette 5mL of the above solution, transfer it to a 25ml volumetric flask, add 1.0mL LaCl 3 solution (mass fraction 10%) and 1.0mL CuSO 4 Solution (mass fraction 15%), constant volume with 1% nitric acid solution, LaCl in the final...

Embodiment 2

[0087] (1) Digestion of samples: Use a pipette to accurately pipette 5mL of rhodium-containing spent catalyst aqueous solution, place it in a 250mL beaker, evaporate it on a heating plate at about 100°C until there is no obvious steam, add 20mL of concentrated sulfuric acid, and heat up temperature for 180 minutes for digestion. After the digestion is completed, continue to heat, evaporate the sulfuric acid to a nearly dry state, add 5mL of concentrated nitric acid after cooling, continue to heat until the solution becomes colorless and transparent, and cool down.

[0088] (2) Test sample preparation: transfer the sample into a 100mL volumetric flask, and dilute to volume with 1% nitric acid solution. Use a pipette to accurately pipette 5mL of the above solution, transfer it to a 25ml volumetric flask, add 1.0mL LaCl 3 solution (mass fraction 10%) and 1.0mL CuSO 4 Solution (mass fraction 15%), constant volume with 1% nitric acid solution, LaCl in the final sample solution 3...

Embodiment 3

[0095] (1) Sample digestion: Use a pipette to accurately pipette 5mL of rhodium-containing catalyst aqueous solution, place it in a 250mL beaker, evaporate it on a heating plate at about 100°C until there is no obvious steam, add 15mL of concentrated sulfuric acid, and raise the heating temperature Digestion was performed for 160 minutes. After the digestion is completed, continue to heat, evaporate the sulfuric acid to a nearly dry state, add 4mL of concentrated nitric acid after cooling, continue to heat until the solution becomes colorless and transparent, and cool down.

[0096] (2) Test sample preparation: transfer the sample into a 100mL volumetric flask, and dilute to volume with 1% nitric acid solution. Use a pipette to accurately pipette 5mL of the above solution, transfer it to a 25ml volumetric flask, add 1.0mL LaCl 3 solution (mass fraction 10%) and 1.0mL CuSO 4 Solution (mass fraction 15%), constant volume with 1% nitric acid solution, LaCl in the final sample s...

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Abstract

The invention discloses a method for detecting rhodium in a water phase of an olefin hydroformylation reaction system catalyzed by a water-soluble rhodium-phosphine complex. A flame atomic absorption method is adopted for qualitative or / and quantitative detection. The method comprises preparation of a test solution, and the test solution contains 2 mg / mL-12 mg / mL of LaCl3 and 2 mg / mL-15 mg / mL of CuSO4. The method is high in determination sensitivity, less in interference, wide in detection range, good in repeatability and low in cost. The effective analysis method is provided for determining the content of rhodium in the aqueous phase of the catalyst in industrial production of a water-organic two-phase catalytic system.

Description

technical field [0001] The invention relates to the field of detection methods for rhodium content in aqueous solutions, in particular to a detection method for rhodium in the water phase of an olefin hydroformylation reaction system catalyzed by a water-soluble rhodium-phosphine complex. Background technique [0002] In the industrial application of water-organic two-phase catalyzed hydroformylation of olefins to prepare aldehydes, the catalyst used is a water-soluble rhodium-phosphine complex. The content of rhodium directly affects the activity of the catalyst, the ratio of the catalyst, the ligand, and the reaction substrate, the efficiency of the aldehyde-forming reaction, and the operating cycle of the equipment. [0003] In the process of olefin hydroformylation to produce aldehydes, the water-organic two-phase solution from the carbonylation reactor enters the chromatographic tank for static phase separation. The lower floor is the water phase that contains water-so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
CPCG01N21/3103
Inventor 陈华向进周凡丁吴前辉
Owner 成都欣华源科技有限责任公司
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